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Ammonia → (+/-)-9-(3-Carbamoyl-3-hydroxy-but-1-ynyl)-8-fluoro-4,5-dihydro-6-oxa-1,3a-diaza-benzo[e]azulene-2-carboxylic acid amide

HRID 575187
ノート
印刷プレビュー

反応式

HRID 575187 の反応式
[C:1]([C:4]1[N:5]=[C:6]2[C:12]3[CH:13]=[C:14]([C:18]#[C:19][C:20]([OH:26])([CH3:25])[C:21](OC)=[O:22])[C:15]([F:17])=[CH:16][C:11]=3[O:10][CH2:9][CH2:8][N:7]2[CH:27]=1)(=[O:3])[NH2:2].OC(C)(C#C)C(OC)=O.BrC1C(F)=CC2OCC[N:44]3C=C(C(N)=O)N=C3C=2C=1.N>CO>[NH2:44][C:21](=[O:22])[C:20]([OH:26])([CH3:25])[C:19]#[C:18][C:14]1[C:15]([F:17])=[CH:16][C:11]2[O:10][CH2:9][CH2:8][N:7]3[CH:27]=[C:4]([C:1]([NH2:2])=[O:3])[N:5]=[C:6]3[C:12]=2[CH:13]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 8669305110-Bromo-9-fluoro-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamideHCID 86693109Methyl 4-(2-carbamoyl-9-fluoro-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepin-10-yl)-2-hydroxy-2-methylbut-3-ynoateHCID 86693195Methyl 2-hydroxy-2-methylbut-3-ynoate

生成物 1

HCID 71715163
(+/-)-9-(3-Carbamoyl-3-hydroxy-but-1-ynyl)-8-fluoro-4,5-dihydro-6-oxa-1,3a-diaza-benzo[e]azulene-2-carboxylic acid amide
収率 15%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

similar to General Procedure M, A solution of methyl 4-(2-carbamoyl-9-fluoro-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepin-10-yl)-2-hydroxy-2-methylbut-3-ynoate (300 mg, 0.80 mmol, 1.00 equiv) (prepared by reaction of methyl 2-hydroxy-2-methylbut-3-ynoate and 10-bromo-9-fluoro-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide in methanol saturated with ammonia (40 mL) was stirred for 12 h at 25° C. The resulting mixture was concentrated under vacuum. The residue was washed with 3×10 mL of methanol and 2×5 mL of CH3CN. The solid was dried in an oven under reduced pressure. This resulted in 43 mg (15%) of the title compound as a brown solid.

後処理

  1. concentrationThe resulting mixture was concentrated under vacuum
  2. washThe residue was washed with 3×10 mL of methanol and 2×5 mL of CH3CN
  3. customThe solid was dried in an oven under reduced pressure

出典と根拠

ORDレコード
ord-8e18aea6610f417abed1d822fdf05173
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09034866B2

反応ノート

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